反应详情

To 1250 ml of dehydrated N,N-dimethylformamide solution containing 63.1 g (1.45 mol) of sodium hydride (55% dispersed material in mineral oil) which had been washed three times with each 500 ml of dehydrated heptane was added dropwise 750 ml of dehydrated N,N-dimethylformamide solution containing 263 g (purity: 95%, 1.36 mol) of ethyl 2-methoxymethyl-1H-pyrrol-3-carboxylate obtained in Reference example 15-(c) at room temperature under argon atmosphere, and the mixture was stirred for 30 minutes. Then, 242 g (1.45 mol) of (2-trimethylsilylethoxy)methyl chloride was added dropwise to the mixture under ice-cooling, and the mixture was further stirred at room temperature for 3 hours. After completion of the reaction, the reaction mixture was poured into ice-water, neutralized with 30% aqueous potassium hydrogen sulfate solution, and extracted with toluene. The organic layer after separation was washed successively with water, and then, with a saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain 420 g (purity: 98.6%) of the title compound as a yellowish oil. (Yield: 96%)

1. washhad been washed three times with each 500 ml of dehydrated heptane
2. additionwas added dropwise 750 ml of dehydrated N,N-dimethylformamide solution
3. customobtained in Reference example 15-(c) at room temperature under argon atmosphere
4. temperaturecooling
5. stirringthe mixture was further stirred at room temperature for 3 hours
6. customAfter completion of the reaction
7. extractionextracted with toluene
8. customThe organic layer after separation
9. washwas washed successively with water
10. dry with materialwith a saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate
11. concentrationconcentrated under reduced pressure